1、Designation: D 7094 04An American National StandardStandard Test Method forFlash Point by Modified Continuously Closed Cup(MCCCFP) Tester1This standard is issued under the fixed designation D 7094; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the flashpoint of fuels, lube oils, solvents
3、and other liquids by acontinuously closed cup tester utilizing a specimen size of 2mL, cup size of 7 mL, with a heating rate of 2.5C per minute.1.1.1 Apparatus requiring a specimen size of 1 mL, cup sizeof 4 mL, and a heating rate of 5.5C per minute must be runaccording to Test Method D 6450.1.2 Thi
4、s flash point test method is a dynamic method anddepends on definite rates of temperature increase. It is one ofthe many flash point test methods available and every flashpoint test method, including this one, is an empirical method.NOTE 1Flash point values are not a constant physical chemicalproper
5、ty of materials tested. They are a function of the apparatus design,the condition of the apparatus used, and the operational procedure carriedout. Flash point can, therefore, only be defined in terms of a standard testmethod and no general valid correlation can be guaranteed between resultsobtained
6、by different test methods or where different test apparatus isspecified.1.3 This test method utilizes a closed but unsealed cup withair injected into the test chamber.1.4 This test method is suitable for testing samples with aflash point from 35 to 225C.NOTE 2Flash point determinations below 35C and
7、 above 225C maybe performed; however, the precision has not been determined below andabove these temperatures.1.5 If the users specification requires a defined flash pointmethod other than this method, neither this method nor anyother test method should be substituted for the prescribed testmethod w
8、ithout obtaining comparative data and an agreementfrom the specifier.1.6 The values stated in SI are to be regarded as standard.Temperatures are in degrees Celsius, pressure in kilo-Pascals.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It i
9、s theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 7.2, 8.5, and 10.1.2.2. Referenced Documents2.1 ASTM Standards:2D93 Test Methods for Fla
10、sh Point by Pensky-MartensClosed Cup TesterD 4057 Practice for Manual Sampling for Petroleum andPetroleum ProductsD 4177 Test Method for Automatic Sampling of Petroleumand Petroleum ProductsD 6450 Test Method for Flash Point by ContinuouslyClosed Cup (CCCFP) TesterD 6708 Practice for Statistical Ass
11、essment and Improve-ment of the Expected Agreement Between Two TestMethods that Purport to Measure the Same Property of aMaterialE 300 Practice for Sampling Industrial Chemicals2.2 ISO Standards:3ISO Guide 34 Quality Systems Guidelines for the Produc-tion of Reference MaterialsISO Guide 35 Certifica
12、tion of Reference MaterialsGeneral and Statistical Principles3. Terminology3.1 Definitions:3.1.1 flash point, nthe lowest temperature corrected to apressure of 101.3 kPa at which application of an ignition1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubr
13、icants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved Nov. 1, 2004. Published November 2004.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume
14、 information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
15、source causes the vapors of a specimen of the sample to ignitemomentarily under specified conditions of the test.3.1.1.1 DiscussionFor the purpose of this test method, thetest specimen is deemed to have flashed when the hot flame ofthe ignited vapor causes an instantaneous pressure increase ofat lea
16、st 20 kPa inside the closed measuring chamber.43.1.2 dynamic, adjthe condition where the vapor abovethe test specimen and the test specimen are not in temperatureequilibrium at the time at which the ignition source is applied.4. Summary of Test Method4.1 The lid of the test chamber is regulated to a
17、 temperatureat least 18C below the expected flash point.A2 6 0.2 mL testspecimen of a sample is introduced into the sample cup. Bothspecimen and cup are at a temperature at least 18C below theexpected flash point; cooled if necessary. The cup is then raisedand pressed onto the lid of specified dimen
18、sions to form thecontinuously closed but unsealed test chamber with an overallvolume of 7.0 6 0.3 mL.4.2 After closing the test chamber, the temperatures of thetest specimen and the regulated lid are allowed to equilibrate towithin 1C. Then the lid is heated at a prescribed, constant rate.For the fl
19、ash tests, a high voltage arc of defined energy isdischarged inside the test chamber at regular intervals. Aftereach ignition, a variable amount of air (see Table 1)isintroduced into the test chamber to provide the necessaryoxygen for the next flash test. The pressure inside the continu-ously closed
20、 but unsealed test chamber remains at ambientbarometric pressure except for the short time during the airintroduction and at a flash point.4.3 After each arc application, the instantaneous pressureincrease above the ambient barometric pressure inside the testchamber is monitored. When the pressure i
21、ncrease exceeds 20kPa, the temperature at that point is recorded as the uncorrectedflash point, which is then corrected to barometric pressure.5. Significance and Use5.1 The flash point temperature is one measure of thetendency of the test specimen to form a flammable mixturewith air under controlle
22、d laboratory conditions. It is only oneof a number of properties which must be considered inassessing the overall flammability hazard of a material.5.2 Flash point is used in shipping and safety regulations todefine flammable and combustible materials and for classifica-tion purposes. This definitio
23、n may vary from regulation toregulation. Consult the particular regulation involved for pre-cise definitions of these classifications.5.3 This test method can be used to measure and describethe properties of materials in response to heat and an ignitionsource under controlled laboratory conditions a
24、nd shall not beused to describe or appraise the fire hazard or fire risk ofmaterials under actual fire conditions. However, results of thistest method may be used as elements of a fire risk assessment,which takes into account all of the factors which are pertinentto an assessment of the fire hazard
25、of a particular end use.5.4 Flash point can also indicate the possible presence ofhighly volatile and flammable materials in a relatively non-volatile or nonflammable material, such as the contaminationof lubricating oils by small amounts of diesel fuel or gasoline.This test method was designed to b
26、e more sensitive to potentialcontamination than Test Method D 6450.6. Apparatus6.1 Flash Point Apparatus, Continuously Closed CupOperationThe type of apparatus suitable for use in this testmethod employs a lid of solid brass, the temperature of whichis controlled electrically. Two temperature sensor
27、s for thespecimen and the lid temperatures, respectively, two arc pinsfor a high voltage arc, and a connecting tube for the pressuremonitoring and the air introduction are incorporated in the lid.Associated equipment for electrically controlling the chambertemperature is used, and a digital readout
28、of the specimentemperature is provided. The apparatus and its critical elementsare shown in Figs. A1.1 and A1.2.56.1.1 Test ChamberThe test chamber is formed by thesample cup and the temperature controlled lid and shall have anoverall volume of 7 6 0.3 mL. A metal to metal contactbetween the lid and
29、 the sample cup shall provide good heatcontact but allow ambient barometric pressure to be maintainedinside the test chamber during the test. Critical dimensions areshown in Fig. A1.2. The pressure inside the measuring cham-ber during the temperature increase is monitored. A seal that istoo tight re
30、sults in a pressure increase above ambient due to thetemperature and the vapor pressure of the sample. A poor heatcontact results in a bigger temperature difference between thesample and the heated lid.6.1.2 Sample CupThe sample cup shall be made ofnickel-plated aluminum or other material with simil
31、ar heatconductivity. It shall have an overall volume of 7 6 0.3 mLandshall be capable of containing 2 6 0.2 mL of sample. Thecritical dimensions and requirements are shown in Fig. A1.2.6.1.3 Specimen Temperature SensorThe specimen tem-perature sensor (Fig. A1.1) shall be a thermocouple (NiCr-Nior si
32、milar) in stainless steel of 1 mm diameter with a response4The method of detecting the flash point by monitoring the instantaneouspressure increase is covered by a patent. Interested parties are invited to submitinformation regarding the identification of an alternative(s) to this patented item toth
33、e ASTM International Headquarters. Your comments will receive careful consid-eration at a meeting of the responsible technical committee, which you may attend.5The sole source of supply of the continuously closed cup testers meeting theserequirements known to the committee at this time are available
34、 from GrabnerInstruments, A-1220 Vienna/Austria, Dr. Otto-Neurath-Gasse 1. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may a
35、ttend.TABLE 1 Volume of Introduced Air as a Function ofSample TemperatureSample TemperatureRange (C)Introduced Volumeof Air (mL)below 80 080 to below 150 0.5 6 0.15150 to below 200 1 6 0.2200 to below 300 1.5 6 0.3300 and above 2 6 0.4D7094042time of t (90) = 3 s. It shall be immersed to a depth of
36、at least2 mm into the specimen. It shall have a resolution of 0.1C anda minimum accuracy of 6 0.2C, preferably with a digitalreadout.6.1.4 Magnetic StirringThe apparatus shall have provi-sions for stirring of the sample. A rotating magnet outside thesample cup shall drive a small stirring magnet whi
37、ch is insertedinto the sample cup after sample introduction. The stirringmagnet shall have a diameter of 3 6 0.2 mm and a length of 126 1 mm. The rotation speed of the driving magnet shall bebetween 250 and 270 rev/min.6.1.5 Air IntroductionThe apparatus shall have provisionsfor introduction of air
38、immediately after each flash test. The airshall be introduced by a short air pulse from a small membranecompressor by means of a T-inlet in the connecting tube to thepressure transducer. The volume of the introduced air, from 0.5to 2 mL, is dependent on the sample temperature (see Table 1).6.1.6 Ele
39、ctrical heating and thermoelectric cooling of the lid(see the Peltier element shown in Fig. A1.1) shall be used toregulate the temperature of the test chamber for the duration ofthe test. The temperature regulation shall have a minimumaccuracy of 6 0.2C.6.1.7 A high voltage electric arc shall be use
40、d for theignition of the flammable vapor. The energy of the arc shall be1.3 6 0.3 J (1.3 6 0.3 Ws) per arc and the energy shall beapplied within 19 6 2 m/s. (WarningBecause samplescontaining low flash material or having a flash point below thepreset initial temperature can oversaturate the vapor ins
41、ide thechamber and hence prohibit the detection of a flash point in thechosen range, a precautionary arc set at 5C intervals isrequired while the lid and sample cup temperatures areequalizing.)6.1.8 The pressure transducer for the flash point detectionshall be connected to the connecting tube in the
42、 lid and shallhave a minimum operational range from 80 to 177 kPa with aminimum resolution of 0.1 kPa and a minimum accuracy of 60.5 kPa. It shall be capable of detecting an instantaneouspressure increase above barometric pressure of a minimum of20 kPa within 100 m/s.NOTE 3The monitoring of the inst
43、antaneous pressure increase abovebarometric pressure is one of several methods to determine a flash insidethe test chamber. A pressure increase of 20 kPa corresponds to a flamevolume of approximately 2.5 mL.NOTE 4An automatic barometric correction, which is performedaccording to the procedure descri
44、bed in 12.1, can be installed in the tester.The absolute pressure reading of the pressure transducer described in 6.1.8may be used for the correction.6.1.9 The introduction of a test specimen of 2.0 6 0.2 mLshall be accomplished by the use of a pipette or syringe of therequired accuracy.7. Reagents
45、and Materials7.1 Purity of ReagentsUse only chemicals of purity speci-fied in Table X1.1. Unless otherwise indicated, it is intendedthat all reagents conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Societywhere such specifications are available.6Other gr
46、ades may beused, provided it is first ascertained that the reagent is ofsufficient purity to permit its use without lessening the accu-racy of the determination.7.1.1 Anisole(WarningSee 7.2.)7.1.2 Dodecane(WarningSee 7.2.)7.2 Cleaning SolventsUse only noncorrosive solvents ca-pable of cleaning the s
47、ample cup and the lid. Two commonlyused solvents are toluene and acetone. (WarningAnisole,dodecane, toluene, acetone, and many solvents are flammableand are health hazards. Dispose of solvents and waste materialin accordance with local regulations.)8. Sampling8.1 Obtain at least a 50 mL sample from
48、a bulk test site inaccordance with the instructions given in Practice D 4057,D 4177,orE 300. Store the sample in a clean, tightly sealedcontainer at a low temperature.8.2 Do not store samples for an extended period of time ingas permeable containers, such as plastic, because volatilematerial may dif
49、fuse through the walls of the container.Discard samples in leaky containers and obtain new samples.8.3 Erroneously high flash points can be obtained whenprecautions are not taken to avoid loss of volatile material. Donot open containers unnecessarily. Do not make a transferunless the sample temperature is at least 18C below theexpected flash point. When possible, perform the flash point asthe first test.8.4 Samples of very viscous materials may be warmed untilthey are reasonably fluid before they are tested. However, donot heat the unsealed sample ab
